반응 #217451

반응 방정식

dimethylformamide

allyl(4-chlorobutyl) ether

4-hydroxybenzoic acid

potassium carbonate

→

4-(4-allyloxybutyloxy)benzoic acid

수율 123.0%

용매

Water

반응 조건

후처리

1. 1
   추출the solution was extracted with toluene
2. 2
   세척The toluene layer was washed well with water
3. 3
   workup.DISTILLATIONtoluene was distilled off
4. 4
   workup.ADDITIONSodium hydroxide 20 g, water 50 ml and ethanol 200 ml were added to the resulting residue
5. 5
   온도refluxed for 2 hours
6. 6
   workup.DISTILLATIONEthanol was distilled off
7. 7
   workup.ADDITIONhydrochloric acid was added to the residue
8. 8
   추출The solution was extracted with diethyl ether
9. 9
   건조the extract was dried on anhydrous magnesium sulfate
10. 10
    기타A residue obtained
11. 11
    workup.DISTILLATIONby distilling the solvent
12. 12
    기타off was recrystallized from a mixed solvent of ethanol and water

실험 절차

A dimethylformamide (50 ml) solution of allyl(4-chlorobutyl) ether 14 g, 4-hydroxybenzoic acid 14 g and potassium carbonate 14 g was stirred at 90° C. for 3 hours. Water was added thereto, and the solution was extracted with toluene. The toluene layer was washed well with water, and then toluene was distilled off. Sodium hydroxide 20 g, water 50 ml and ethanol 200 ml were added to the resulting residue and refluxed for 2 hours. Ethanol was distilled off, and then hydrochloric acid was added to the residue to acidify the solution. The solution was extracted with diethyl ether, and the extract was dried on anhydrous magnesium sulfate. A residue obtained by distilling the solvent off was recrystallized from a mixed solvent of ethanol and water to obtain 29 g of 4-(4-allyloxybutyloxy)benzoic acid. Phase transition temperature: C94N107I.

출처